The method of obtaining trinational salt nitrilotriethanol acid


(57) Abstract:

The inventive product: trinacria Sol nitrilotriethanol acid, BF C3H9NaNO9P3. Reagent I: ammonia water. Reagent 2: formalin. Reagent 3: PCl3. Reaction conditions: the resulting product is treated with sodium hydroxide at 70 - 80oWith up to pH environment of 3.5 to-4.5, followed by separation of the target product by filtration. 1 C. p. F.-ly, 2 tab.

The invention relates to a technology for sodium salts of nitrilotriethanol acid (NTF), used as components of detergents, inhibitors, and other industries.

Known methods for producing sodium salts NTF (mostly five - and destinationy) in aqueous solution by neutralizing with caustic soda, the reaction mass formed in obtaining NTF interaction of phosphorus compounds (phosphorous acid, phosphorus trichloride or monomethylfumarate) with ammonia and formaldehyde in the aquatic environment.

However, the use of sodium salts NTF in the form of aqueous solutions often is-low-tech, for example, in those processes where it is undesirable introduction of water, Lucene sodium salts NTF in solid form is unknown.

To obtain trinational salt NTF proposed reaction mass formed by the interaction of phosphorus trichloride, ammonia and formaldehyde and containing NTF in the amount of 40-50 wt. neutralize with sodium hydroxide solution at a temperature of 70-80aboutWith up to pH 3.5-4.5. After cooling to 25-30aboutWith precipitation trinational salt NTF dowdney, which is filtered off. In addition, to use the properties of Na3NTF remaining in the mother solution, to improve the overall yield of Na3NTF in the mother liquor add 1-5 wt. oksietilidendifosfonovaya acid (HEDP) (TU 6-02-1251-81 with ISM. 1,2) adjusted with sodium hydroxide solution to pH 4.5-5.5.

The chemistry of the process describes a General scheme:

[NH3]+3CH2O+3PCl3+6H2O +9HCl

As [NH3] may apply ammonia ammonia water, methenamine, ammonium chloride.

The invention is illustrated by the following examples.

P R I m e R 1. In chetyrehosnuju flask with a capacity of 1 DM3, equipped with a mechanical stirrer, a refrigerator connected to a absorption of hydrogen chloride, and two drip funnels, placed 108 g of 36% hydrochloric acid, then with vigorous paramesh g of 37% formalin solution (1.8 M CH2O) and 40 g of ammonia water (0.6 M NH3), maintaining a given temperature the rate of addition of reagents and external cooling. Upon completion of addition, the reaction mass is heated to 100aboutC and maintained at this temperature for 1 h for a more complete removal of released hydrogen chloride; by the end of the exposure the content of the NTF in the reaction mass is on the analytical data to 42.5 wt. (125,6 g). Then the reaction mass to cool slightly and with vigorous stirring, added dropwise 44% caustic soda solution with such a speed that the temperature of the reaction mass was 70aboutC. the Dosage of caustic soda stop when the pH reaches a 3.5. After the reaction mass is then cooled to 25-30aboutC; the resulting suspension is easily filtered. Obtained crystalline precipitate in the amount of 101 g (53.6%,]. counting on l3). Analytical data content trinational salt NTF dowdney 96.5 wt.

The mother solution, resulting in 335 g containing analytical data 21 wt. Na3NTF, processed, as shown below in examples 7-10.

P R I m e R s 2-6. Obtaining the reaction mass containing the NTF, the GLA. 1.

P R I m e R s 7-10. To 100 g of the mother liquor obtained in the conditions of example 1, was added with stirring eddc, then 44% sodium hydroxide solution to pH 4.5-5.5, maintaining the temperature at 25-30aboutC. conditions of processing of the mother liquor and analytical characteristics of the finished product are shown in table. 2.

As examples (PL. 1), the process of neutralization of the reaction mixture containing the NTF at a temperature below 70about(Example 2) leads to the formation of poorly filterable viscous pasty mass, and the time of filtration is increased up to several hours, which is connected, apparently, with the fact that at temperatures below 70aboutWith along with education trinational salt NTF rapid coprecipitation the NTF-acid.

From the examples in the table. 1, it is seen that at the termination of the neutralization of the reaction mixture at pH below 3.5 (example 4) significantly reduced the yield of crystalline salt NTF because of incomplete neutralization, and at pH higher than 4.5 (example 5) due to the dissolution of already precipitated salt.

As the table shows. 2 (example 7), the mother liquor after filtration, containing 17-21% Na3NTF is unstable after some hundred is emery 8, 9) prevents precipitation upon standing and makes it sustainable. When the content eddc above 5 wt. (example 10) starts the deposition of poorly soluble trinational salt of HEDP. Processing of the mother liquor caustic soda to pH 4.5-5.5 required, since at pH below 4.5 liquid product is corrosive materials, packaging and equipment that makes its transportation and storage.

Thus, the proposed method allows for the first time to get chinatravel salt NTF in crystalline form with a yield of about 55% of theoretical. At the same time the proposed method of stabilizing the mother liquor after filtration of the solid salt NTF, allows the properties of Na3NTF, contained in the number 17-21 wt. turning thus the production waste into marketable products designed for use in those industries that use sodium salt NTF, for example, as an additive to synthetic detergents.

1. The METHOD of OBTAINING TRINATIONAL SALT NITRILOTRIETHANOL ACID, characterized in that the ammonia water is subjected to interaction with formalin and phosphorus trichloride followed by treatment of the resulting product ekipa p. 1, characterized in that the mother liquor after filtration with a mass fraction trinational salt nitrilotriethanol acid 17 to 21 wt. % handle 1 to 5 wt.% oksietilidendifosfonovaya acid and alkalinized with caustic soda to a pH of 4.5 to 5.5.


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